CN107946638A - Lithium ion battery containing manganese-based positive electrode material - Google Patents
Lithium ion battery containing manganese-based positive electrode material Download PDFInfo
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- CN107946638A CN107946638A CN201711306610.4A CN201711306610A CN107946638A CN 107946638 A CN107946638 A CN 107946638A CN 201711306610 A CN201711306610 A CN 201711306610A CN 107946638 A CN107946638 A CN 107946638A
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- manganese
- lithium
- electrode material
- ion battery
- lithium ion
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a lithium ion battery containing a manganese-based anode material, which comprises an anode material, a cathode material, a diaphragm and electrolyte containing manganese ions, wherein the anode material is a spinel-type, layered or olivine-type manganese-based material, the cathode material is lithium metal, a cathode based on de-intercalation reaction, a cathode based on alloy reaction or a cathode based on conversion reaction, and the preparation method of the electrolyte containing the manganese ions comprises the following steps: and dissolving a manganese salt crystal in an electrolyte containing a lithium salt and an organic solvent to obtain the electrolyte containing manganese ions, wherein the manganese salt crystal is one or more of manganese nitrate, manganese acetate and manganese sulfate, and the lithium salt is selected from lithium hexafluorophosphate, lithium perchlorate or lithium bistrifluoromethanesulfonylimide. In the lithium ion battery, the spinel type lithium manganate electrode has good high-temperature electrochemical performance, and the battery has simple preparation process, low cost and strong application value.
Description
Technical Field
The invention relates to the technical field of battery preparation, in particular to a lithium ion battery containing a spinel type lithium manganate electrode.
Background
With the increasing popularity of portable electronic products such as notebook computers and mobile phones, and the development of electric vehicles and energy storage batteries, people have made higher demands on various aspects such as energy density, service life and cost of power supplies. Lithium ion batteries, which are small in size, light in weight, environmentally friendly, and high in specific energy, are widely used and are gradually replacing more traditional batteries, such as zinc-manganese batteries, lead-acid batteries, cadmium-nickel batteries, and metal hydride batteries. As a new generation of high-energy power source, lithium ion batteries have been developed in compliance with the needs of economic development, resource utilization, and environmental protection.
Lithium ion batteries currently commercialized mainly use lithium cobaltate (LiCoO) 2 ) Lithium cobaltate is excellent in electrochemical properties as an electrode material, but it is expensive, low in potential, and toxic in cobalt compounds as an electrode material. In order to avoid the above-mentioned disadvantages of lithium cobaltate, manganese-based lithium metal oxide electrode materials have come into use. Among such oxides, the simplest one that can be prepared is represented by manganese-based spinel-type lithium manganate (LiMn) 2 O 4 ). The spinel type lithium manganate has a three-dimensional lithium ion channel, has the advantages of low price, high potential, environmental friendliness, high safety performance and the like when being used as an electrode material, and is a positive electrode material which is hopeful to replace lithium cobaltate to become a new generation of lithium ion batteries. However, liMn 2 O 4 The electrochemical stability at high temperature is poor, which also limits its industrialization.
To improve spinel type LiMn 2 O 4 The lack of high temperature stability makes it possible to dope the material on the one hand. B, al, si, ge, etc. may be used as the doping element. On the other hand, the salt of Zn, mg or the like may be used in LiMn 2 O 4 The surface of (2) is coated. Although these methods can improve spinel-type LiMn 2 O 4 But the processes involved in these methods are expensive, complicated, and even somewhat complexSome of the required elements are toxic, which is detrimental to LiMn instead 2 O 4 Commercialization of electrode materials.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide the lithium ion battery containing the manganese-based cathode material.
The invention provides a lithium ion battery containing a manganese-based anode material, which comprises an anode material, a cathode material, a diaphragm and electrolyte containing manganese ions, wherein the anode material is a spinel-type, layered or olivine-type manganese-based material, the cathode material is lithium metal, a cathode based on de-intercalation reaction, a cathode based on alloy reaction or a cathode based on conversion reaction, and the preparation method of the electrolyte containing the manganese ions comprises the following steps: dissolving manganese salt crystals in an electrolyte containing lithium salt and an organic solvent to obtain an electrolyte containing manganese ions, wherein the manganese salt crystals are manganese nitrate (Mn (NO) 3 ) 2 ) Manganese acetate (Mn (CH) 3 COO) 2 ) And manganese sulfate (MnSO) 4 ) One or more of the above, and the lithium salt is selected from lithium hexafluorophosphate (LiPF) 6 ) Lithium perchlorate or lithium bistrifluoromethanesulfonylimide.
In the system of manganese-based positive electrode materials, the inevitable presence of Mn 3+ Is formed of Mn 3+ Disproportionation reaction to produce Mn 4+ And Mn 2+ In which Mn is 2+ Will dissolve in the electrolyte, causing irreversible loss of battery capacity, and also causing collapse of manganese-based material structure, thereby gradually deteriorating electrochemical performance, which is particularly significant under high temperature conditions. The invention uses manganese salt crystals such as manganese nitrate and the like as additives, and manganese ions (Mn) in electrolyte 2+ ) Can effectively inhibit Mn 3+ The disproportionation reaction ensures the stability of the structure, thereby improving the high-temperature performance of the structure.
Further, the cathode material is spinel lithium manganate (LiMn) 2 O 4 ) Spinel type lithium nickel manganese oxide(LiNi 0.5 Mn 1.5 O 4 ) Layered lithium nickel manganese oxide (LiNi) 0.5 Mn 0.5 O 2 ) Or olivine-type lithium manganese phosphate (LiMnPO) 4 ). Preferably, the cathode material is spinel type lithium manganate (LiMn) 2 O 4 )。
Further, the negative electrode material is lithium metal, negative electrode Li based on deintercalation reaction 4 Ti 5 O 12 Negative electrode Sn based on alloying reaction, or negative electrode Co based on conversion reaction 3 O 4 Or manganese oxide (Mn) x O y ). Preferably, the anode material is lithium metal.
Preferably, the manganese salt crystal is manganese nitrate.
Furthermore, the concentration of the manganese ions in the electrolyte containing the manganese ions is 0.0001-0.01 mol/L. Preferably, the concentration of manganese ions is 0.001mol/L. The method and the device use lower concentration of manganese ions to achieve better effect, and are beneficial to saving resources and maximizing utilization.
The reason why the concentration of manganese ions is set is as follows: on one hand, if the concentration is too high, manganese ions can be excessively deposited on the negative electrode to damage the negative electrode material, and the lithium ions are prevented from being extracted from the negative electrode; on the other hand, the manganese ions in the lithium manganate have low concentration 3+ The suppression of disproportionation reaction is weakened and thus the optimum effect cannot be achieved.
Further, the concentration of the lithium salt in the electrolyte containing the lithium salt and the organic solvent is 0.8 to 2.2mol/L.
Further, the organic solvent is one or more of Ethylene Carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC), polycarbonate (PC), tetraglyme (G4), dioxolane (DOL), and Triglyme (TEGDME).
Preferably, the organic solvent is Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a 1.
Further, the preparation of the electrolyte containing manganese ions further comprises the step of removing water in the electrolyte containing manganese ions so that the water content therein is less than 100 ppm.
Further, adding a molecular sieve into the electrolyte containing manganese ions to remove water.
Further, the lithium ion battery is a button battery, a soft package battery or a cylindrical battery.
Further, the positive electrode material also includes acetylene black and Polytetrafluoroethylene (PTFE).
Further, the diaphragm is a glass fiber film, a polyethylene microporous film, a polypropylene microporous film or an ethylene-propylene copolymer microporous film.
By the scheme, the invention at least has the following advantages:
in the lithium ion battery, the manganese-based positive electrode material has extremely high electrochemical stability at high temperature (50-65 ℃), and can obviously inhibit Mn in the material in a high-temperature environment 3+ Thereby remarkably improving the electrochemical performance of the electrolyte. At 55 ℃ and 2C (1C=148mAg) -1 ) In a half-cell test of multiplying power, after 200 cycles, the discharge capacity of a half-cell prepared by using the electrolyte containing manganese ions is still more than 80% of the initial discharge capacity.
The lithium ion battery of the invention has simple preparation process and low cost.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a charge-discharge curve of a half cell in example 1;
fig. 2 is a charge-discharge curve of a half cell in example 2 of the invention;
figure 3 is a graph comparing the cycling performance of the half cells of examples 1 and 2.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The present embodiment provides a lithium ion battery as a control experiment, and the preparation method thereof is as follows:
mixing LiMn 2 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling on a glass plate to form a film, and cutting into a circular sheet with the diameter of 12 mm; the above-mentioned disk is compacted on an aluminum net and dried overnight in a vacuum drying oven at 100 ℃ to be used as a positive electrode material of a battery. Mixing LiPF 6 Dissolved in EC and DEC (volume ratio = 1), as an electrolyte (LiPF in electrolyte 6 The concentration is 1mol L -1 ) And assembling the positive electrode material, the negative electrode material and the electrolyte into a half cell by using glass fiber as a diaphragm.
The charging and discharging curve is tested under the conditions of 55 ℃,2C multiplying power and 3.3-4.3V charging and discharging window, and the result is shown in figure 1. The first circle discharge capacity is less than 100mAh g -1 After 100 cycles, the capacity rapidly decayed to 55mAh g -1 The capacity retention ratio at 100 cycles was only about 50%. During subsequent cycles, the capacity is still visibly fading.
Example 2
The present embodiment provides a lithium ion battery of the present invention, and a preparation method thereof is as follows:
mixing spinel type LiMn 2 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling the mixture on a glass plate to form a film, and cutting the film into a wafer with the diameter of 12 mm; the above-mentioned disk is compacted on an aluminum net and dried overnight in a vacuum drying oven at 100 ℃ to be used as a positive electrode material of a battery. Mixing LiPF 6 Dissolved in EC and DEC (volume ratio = 1), while manganese nitrate (Mn (NO 3 ) 2 ) And dissolved to obtain an electrolyte (Mn (NO) in the electrolyte 3 ) 2 The concentration is 0.001mol L -1 ，LiPF 6 The concentration is 1mol L -1 ) And assembling the positive electrode material, the negative electrode material and the electrolyte into a half cell by using glass fiber as a diaphragm.
The charging and discharging curve is tested under the conditions of 55 ℃,2C multiplying power and 3.3-4.3V charging and discharging window, and the result is shown in figure 2. The first-ring discharge capacity is 110mAh g -1 The first 20 turns all maintain good stability. After 100 circles, the capacity is still kept at 95mAh g -1 The capacity retention ratio at 100 cycles was only about 86%.
In this embodiment, manganese nitrate is used as an electrolyte additive, and the high-temperature stability of spinel lithium manganate can be greatly improved. The method is based on mature electrolyte, has low cost, uses manganese nitrate as an additive, and is convenient and quick to operate. Referring to fig. 1 and 2, the battery capacity of example 1 decayed very rapidly in the high temperature and high current test (fig. 1), while the charge and discharge performance of the battery of example 2 containing the manganese nitrate electrolyte was significantly improved (fig. 2).
Fig. 3 is a graph comparing the cycling performance of the cells under the test conditions of examples 1 and 2. As can be seen from the figure, the performance of the lithium manganate without additive is greatly reduced in the initial stage, and the whole process is smoother after the additive is added. More obviously, after 400 circles, the capacity retention rate of the lithium manganate without the additive is only 40%, compared with the capacity retention rate of the lithium manganate without the additive, the capacity retention rate of the lithium manganate with the additive is more than 70%, and the discharge capacity of the lithium manganate is more than 2 times of that of the lithium manganate without the additive, so that the lithium manganate shows obvious advantages after the additive is added.
Example 3
Mixing spinel type LiMn 2 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling the mixture on a glass plate to form a film, and cutting the film into a wafer with the diameter of 12 mm; the round piece is compacted on an aluminum net and is dried in a vacuum drying oven at 100 ℃ overnight to be used as the anode material of the battery. Mixing LiPF 6 Dissolved in EC and DEC (volume ratio = 1), while manganese sulfate was added thereto,dissolving to obtain electrolyte (MnSO in the electrolyte) 4 The concentration is 0.001mol L -1 ，LiPF 6 The concentration is 1mol L -1 ) And assembling the positive electrode material, the negative electrode material and the electrolyte into a half cell by using glass fiber as a diaphragm.
Example 4
Mixing spinel type LiMn 2 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling on a glass plate to form a film, and cutting into a circular sheet with the diameter of 12 mm; the above-mentioned disk is compacted on an aluminum net and dried overnight in a vacuum drying oven at 100 ℃ to be used as a positive electrode material of a battery. Mixing LiPF 6 Dissolved in EC and DEC (volume ratio = 1), manganese nitrate was added thereto at the same time, and the solution was dissolved to obtain an electrolyte (Mn (NO 3 ) 2 The concentration is 0.01mol L -1 ，LiPF 6 The concentration is 1.5mol L -1 ) And assembling the positive electrode material, the negative electrode material and the electrolyte into a half-cell by taking the celgard diaphragm as the diaphragm.
Example 5
Mixing spinel type LiMn 2 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling on a glass plate to form a film, and cutting into a circular sheet with the diameter of 12 mm; the above-mentioned disk is compacted on an aluminum net and dried overnight in a vacuum drying oven at 100 ℃ to be used as a positive electrode material of a battery. Lithium bistrifluoromethanesulfonimide was dissolved in DMC/PC (volume ratio = 1), and manganese nitrate was added thereto, and the solution was dissolved to obtain an electrolyte (Mn (NO in electrolyte) 3 ) 2 The concentration is 0.001mol L -1 Lithium salt concentration of 2mol L -1 ) And assembling the positive electrode material, the negative electrode material and the electrolyte into a half-cell by taking the celgard diaphragm as the diaphragm.
Example 6
Reacting spinel-type LiNi 0.5 Mn 1.5 O 4 Mixing acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 80: 10, uniformly stirring, uniformly rolling the mixture on a glass plate to form a film, and cutting the film into a wafer with the diameter of 12 mm; the above-mentioned disk is compacted on an aluminum net and dried overnight in a vacuum drying oven at 100 ℃ to be used as a positive electrode material of a battery. Mixing LiPF 6 Dissolved in EC and DEC (volume ratio = 1), manganese nitrate was added thereto at the same time, and the solution was dissolved to obtain an electrolyte (Mn (NO 3 ) 2 The concentration is 0.0001mol L -1 ，LiPF 6 The concentration is 1mol L -1 ) And assembling the anode material, the cathode material and the electrolyte into a half-cell by taking the celgard diaphragm as the diaphragm.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A lithium ion battery containing a manganese-based positive electrode material is characterized in that: the preparation method of the electrolyte containing the manganese ions comprises the following steps of:
dissolving a manganese salt crystal in an electrolyte containing lithium salt and an organic solvent to obtain the electrolyte containing manganese ions, wherein the manganese salt crystal is one or more of manganese nitrate, manganese acetate and manganese sulfate, and the lithium salt is selected from lithium hexafluorophosphate, lithium perchlorate or lithium bistrifluoromethanesulfonylimide.
2. The lithium ion battery comprising a manganese-based positive electrode material according to claim 1, wherein: the anode material is spinel LiMn 2 O 4 Spinel-type LiNi 0.5 Mn 1.5 O 4 Layered LiNi 0.5 Mn 0.5 O 2 Or olivine type LiMnPO 4 。
3. The lithium ion battery containing a manganese-based positive electrode material according to claim 1, characterized in that: the negative electrode material is lithium metal and Li 4 Ti 5 O 12 、Sn、Co 3 O 4 Or manganese oxide.
4. The lithium ion battery comprising a manganese-based positive electrode material according to claim 1, wherein: the concentration of the manganese ions in the electrolyte containing the manganese ions is 0.0001-0.01 mol/L.
5. The lithium ion battery containing the manganese-based positive electrode material of claim 1, wherein: the concentration of the lithium salt in the electrolyte containing the lithium salt and the organic solvent is 0.8-2.2mol/L.
6. The lithium ion battery containing a manganese-based positive electrode material according to claim 1, characterized in that: the organic solvent is one or more of ethylene carbonate, diethyl carbonate, dimethyl carbonate, polycarbonate, tetraethylene glycol dimethyl ether, dioxolane and triethylene glycol dimethyl ether.
7. The lithium ion battery containing a manganese-based positive electrode material according to claim 1, characterized in that: the preparation method of the electrolyte containing the manganese ions further comprises the step of removing water in the electrolyte containing the manganese ions, so that the water content in the electrolyte is below 100 ppm.
8. The lithium ion battery comprising a manganese-based positive electrode material according to claim 1, wherein: the lithium ion battery is a button battery, a soft package battery or a cylindrical battery.
9. The lithium ion battery comprising a manganese-based positive electrode material according to claim 1, wherein: the diaphragm is a glass fiber film, a polyethylene microporous film, a polypropylene microporous film or an ethylene-propylene copolymer microporous film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111740165A (en) * | 2020-06-28 | 2020-10-02 | 宁德新能源科技有限公司 | Electrolyte solution, electrochemical device containing electrolyte solution, and electronic device |
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| US20010046626A1 (en) * | 2000-04-25 | 2001-11-29 | Sanyo Electric Co., Ltd. | Lithium secondary battery |
| JP2010044883A (en) * | 2008-08-08 | 2010-02-25 | Mitsui Chemicals Inc | Nonaqueous electrolyte and lithium secondary battery |
| CN104934639A (en) * | 2015-04-29 | 2015-09-23 | 张家港智电芳华蓄电研究所有限公司 | Preparation method of lithium ion battery electrolyte solution |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010046626A1 (en) * | 2000-04-25 | 2001-11-29 | Sanyo Electric Co., Ltd. | Lithium secondary battery |
| JP2010044883A (en) * | 2008-08-08 | 2010-02-25 | Mitsui Chemicals Inc | Nonaqueous electrolyte and lithium secondary battery |
| CN104934639A (en) * | 2015-04-29 | 2015-09-23 | 张家港智电芳华蓄电研究所有限公司 | Preparation method of lithium ion battery electrolyte solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111740165A (en) * | 2020-06-28 | 2020-10-02 | 宁德新能源科技有限公司 | Electrolyte solution, electrochemical device containing electrolyte solution, and electronic device |
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Application publication date: 20180420 |